関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (4-Phenylcyclohexyl) acetate | HCID 226557 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | HCID 178418412 | HCID 178418412 | — |
反応手順
A solution of 24.3 g (0.11 mol) of O-acetyl-4-phenylcyclohexanol in 1300 ml of methylene chloride is combined with 26.0 g (0.86 mol) of paraformaldehyde and 26.0 g (0.19 mol) of zinc chloride. Hydrogen chloride is introduced into this suspension, with stirring, for 2.5 hours, whilst the temperature rises to about 30° C. and a substantially homogeneous solution is formed. The mixture is then allowed to react for 15 hours at ambient temperature and the reaction mixture is then hydrolysed with stirring in about 1.5 litres of ice water. The organic phase is separated off, the aqueous phase is extracted with methylene chloride again and the two organic phases are combined. They are washed until neutral, dried and evaporated in vacuo. The yellow oil remaining is crystallised by trituration with diisopropylether and the solid product is recrystallised from diisopropylether. White crystals are obtained, melting point 87°-89° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05726205 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-989f1c45e316471198b7f2d873102bdb |
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| 出典メモ | uspto-grants-1998_03 |
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